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Three-dimensional hierarchical SnO 2 microspheres were successfully synthesized through a rapid sonochemical reaction followed by a facile solvothermal process. The resultant samples were characterized in detail by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM). It was observed that the hierarchical SnO 2 microspheres (∼2.2 μm) consist of nanoparticles (∼23–30 nm). These samples are used to fabricate photoelectrodes for dye-sensitized solar cells (DSSCs). The effects of different samples on the photovoltaic performance were studied based on photocurrent-voltage ( J – V ), intensity-modulated photocurrent spectroscopy (IMPS) and intensity-modulated voltage spectroscopy (IMVS). It is found that the highest power conversion efficiency of 6.25% has been achieved based on the hierarchical SnO 2 microspheres film photoanode with thickness of ∼13.5 μm, and the corresponding photovoltaic parameters are 14.11 mA cm −2 in short-circuit current density, 803 mV in open-circuit voltage and 0.55 in fill factor, respectively. [ABSTRACT FROM AUTHOR]